An analytical multi-residue method using gas chromatography coupled with electron capture and a nitrogen-phosphorus detector was investigated for the simultaneous determination of 18 commonly used insecticides and fungicides in Korean ginseng (Panax ginseng C. A. Meyer). Samples were previously extracted with an acetonitrile and cleaned up by solid-phase extraction (SPE). The calibration curves were linear, with determination coefficients higher than 0.989. Recoveries at concentrations between 0.01 and 14.9 ppm ranged from 72.3 to 117.2%, with precision, which was expressed as relative standard deviation (RSD), at values lower than 5%. The proposed method was applied to the determination of pesticide levels from 12 ginseng samples, taken from four different agricultural areas of Jeonnam province, where several insecticides and fungicides were applied. Except in one sample, tolclofos-m was the only pesticide contained at a level lower than the maximum residue limits (MRL) authorized by the Korea Food and Drug Administration (KFDA) in real ginseng samples grown for 4, 5 and 6 years.
An analytical procedure using accelerated solvent extraction and gas chromatography with an electron capture detector has been optimized to simultaneously determine the residue of two insecticides (diazinon and EPN) and one fungicide (isoprothiolane) in polished rice and was confirmed by GC-mass spectrometry. Several parameters, including temperature, pressure, solvent ratio, cell size and cell cycle, were thoroughly investigated to find the optimal extraction conditions. The average recoveries of the three pesticides were between 82.7 and 126.4% at spiking levels of 0.1 and 0.5 ppm. The relative standard deviations were less than 7% for all of the recovery tests. The optimum accelerated solvent extraction operating conditions were 100 degrees C, 1500 atm, acetone-n-hexane (20:80 v/v) as the extraction solvent, two cycles, and a cell size of 33 ml. The total extraction time was approximately 20 min. The optimized procedure has also been applied to the determination of diazinon, isoprothiolane and EPN in real rice samples. In conclusion, accelerated solvent extraction was used for the first time for the analysis of diazinon, isoprothiolane and EPN in polished rice and offers the possibility of a fast and simple process for obtaining a quantitative extraction of the studied pesticides.
A fast and simple high-performance liquid chromatography (HPLC) method for the simultaneous determination of four pesticides having fungicide properties has been proposed for Panax ginseng, C. A. Meyer grown for 4, 5, or 6 years. Analytical separation was performed on C18 columns using ultraviolet detector under gradient conditions. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The HPLC response for all pesticides was linear, with determination coefficients > 0.9986. The average rate of recovery for pesticides spiked with 2 fortification levels was > 72% with relative standard deviations < 9%. The limits of quantification (LOQ) ranged from 0.03 to 0.16 ppm. These LOQs were lower than the respective maximum residue limits (MRL) established by the Korean Food and Drug Administration (KFDA), except for cyazofamid. The proposed method was used to determine pesticide residue levels in samples of ginseng obtained from Jeonnam Province (Republic of Korea). None of the pesticides were found in ginseng samples grown for 4, 5, or 6 years.
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